JP2023539007A - Laboratory-based 3D scanning X-ray Laue microdiffraction system and method (LAB3DμXRD) - Google Patents

Abstract

A collection optic, a sample to be characterized located at a distance from the collection optic, a laboratory x-ray source, a stage for translating and rotating the sample, and a Laue diffraction pattern of the diffracted x-rays. and a detector configured to detect. The sample is translated relative to the focused beam at different rotations, each voxel in the layer is illuminated in more than one rotation, and the Laue diffraction pattern recorded at the different rotations is used to index each voxel in the layer. A method comprising scanning each layer of the sample by scanning. By repeating the translation and rotation of different layers of the sample, a 3D image of the grain structure of the sample is reconstructed. [Selection diagram] Figure 1

Description

The present invention relates to the general field of characterization of crystalline materials using diffraction measurements.

Characterization of crystalline materials helps scientists in both industry and academia understand the properties of crystalline materials and the relationship between processing/manufacturing and properties/performance. Characterization of crystalline materials is performed by characterizing the crystal orientation of each crystal (also called a grain) in a polycrystalline material using diffraction measurements, in which a beam is diffracted from individual grains and the diffraction pattern is recorded. Imaging of the 3D distribution of particle orientation is necessary to fully characterize the sample.

3D Pass through the sample through a depth of millimeters. In 3DXRD experiments, tomographic data acquisition routines are applied using layer beams or box beams that illuminate a cross section or volume of the sample, respectively. High-energy X-ray diffraction microscopy and diffraction contrast tomography (DCT) are offshoot techniques of 3DXRD, which characterizes particles larger than a few μm with spatial resolution down to about 300 nm and standard resolution of about 1 μm. can be evaluated. Currently, it remains difficult to characterize deformed materials and provide local intragranular strain information using 3DXRD.

Scanning 3DXRD can be used to increase spatial resolution and characterize local strain information using a focused monochromatic beam in which the sample volume is mapped after a series of translation and rotation steps. In all of the above cases, if monochromatic X-rays are used, the diffraction will be Bragg diffraction.

Another form of synchrotron 3D characterization is the Laue microdiffraction technique, in which polychromatic X-rays are focused by a non-dispersive Kirkpatrick-Baez mirror to a size of approximately 0.5 μm and directed toward the sample. It will be done. A Pt wire or knife edge is used as a differential aperture to resolve where Laue diffraction occurs along the beam within the sample. 3D volumetric mapping is achieved after the sample is translated horizontally and vertically. In the case of the Laue microdiffraction technique, no rotation of the sample is required.

One limitation of these techniques is that they require synchrotron equipment that is expensive to construct and can only operate with limited beam time. In order to enable faster and cheaper material characterization, it is essential that the systems and techniques described above be adapted for use with X-rays from laboratory radiation sources. So far, only one such system has been developed, namely the LabDCT system. LabDCT systems are disclosed in US Pat. No. 8,385,503 (B2) and US Pat. No. 9,383,324 (B2).

No. 8,385,503 (B2) and US Pat. No. 9,383,324 (B2) or US Patent Application No. 2015/0316493 (A1) discloses that A system is disclosed in which polychromatic divergent light is directed through an aperture to a sample. In this system, specimen translation is performed for specimen alignment. The x-ray beam directed at the sample diverges so that a constant volume of the sample is illuminated. The sample rotates only during LabDCT data acquisition, so LabDCT operates with an aperture that confines the polychromatic conical X-ray beam to the desired volume. By rotating the sample, multiple diffraction spots from different crystal lattice planes of the same particle can be recorded on the area detector with a high signal-to-noise ratio. The spots are used for crystallographic orientation indexing and 3D sample volume reconstruction. However, measurement of stress is not currently possible.

LabDCT operates using a laboratory X-ray source, but has inherent limitations due to the Laue focusing effect and requires that the crystals/particles be free of defects. Furthermore, LabDCT can only 3D map particles with a spatial resolution of 5-10 μm and is only compatible with particles larger than 20-30 μm. This is not sufficient as the typical particle size for most metals is in the range of 1-25 μm. Additionally, LabDCT cannot characterize deformed materials or determine local lattice strains within individual particles.

WO 2009/126868 (A1) brochure focuses monochromatic X-rays, or with a limited range of discretized energies, but as described in US Pat. discloses an x-ray generation system that uses x-rays that are not in the continuous polychromatic spectrum, which would be considered too low for DCT. DCT was originally designed based on a monochromatic synchrotron x-ray beam.

Improved laboratory-based diffraction systems and methods would therefore be advantageous, especially those capable of characterizing particles as small as a few μm in size, in addition to being able to determine local lattice strains. Systems and methods that remain effective even when the sample is deformed would be advantageous.

The project leading to this application has received funding from the European Research Council (ERC) under the European Union's Horizon 2020 research and innovation program (grant agreement number 788567).

Another object of the invention is to provide an alternative to the prior art.

In particular, the object of the present invention is to solve the above-mentioned problems of the prior art, allowing the characterization of small particles with a particle size of the order of a few μm, the determination of local lattice strains, and the characterization of deformed samples. It may be considered to provide a laboratory-based 3D scanning X-ray Laue microdiffraction system.

Accordingly, the above objects and several others are obtained in a first aspect of the present invention by providing a laboratory-based 3D scanning X-ray Laue microdiffraction system for characterizing crystalline materials. The laboratory-based 3D scanning X-ray Laue microdiffraction system is intended to be
- condensing optics;
- material to be characterized during use of the system, which can be placed at a distance from the collection optics;
- a laboratory X-ray source capable of producing a polychromatic X-ray beam;
- a focusing optic is placed in the path of the beam between the X-ray source and the sample and is capable of producing a focused beam with a spot diameter of less than 30 μm at the imaging point in the sample; can be diffracted within the sample from the internal sample volume illuminated by the beam to produce diffracted X-rays;
- a stage for holding a sample, the stage being configurable to rotate and translate the sample at specific distances and angles relative to the focused beam to change the internal sample volume position within the sample;
- a detector configurable to detect a Laue diffraction pattern of diffracted X-rays.

In some embodiments, the detector is a 2D detector.

In a second aspect, the invention further relates to a method for producing 3D orientation imaging of a crystalline material, which may include:
- focusing a polychromatic X-ray beam generated by a laboratory X-ray source to a spot diameter of less than 30 μm in the sample to produce a focused beam;
- defining a first translation axis that may be perpendicular to the beam;
- defining a second translation axis that may be perpendicular to the first translation axis and the beam;
- defining one or more layers within a predetermined gauge volume of the sample along a second translational axis;
- scanning each layer of the sample by translating the sample along a first translational axis and recording the resulting Laue diffraction pattern for each translation;
- irradiating each voxel of the layer in more than one revolution, such that each layer of the sample can be scanned in different rotations of the sample, so that the Laue diffraction pattern consisting of each voxel is recorded in at least two recordings; can,
the layer is scanned by translating the sample to the next layer along a second translational axis;
- indexing the Laue diffraction pattern using the recorded Laue diffraction pattern, preferably reconstructing a 3D image by indexing each voxel within a gauge volume of the grain structure of the sample;

We have determined that by combining scanning 3DXRD and Laue microdiffraction techniques, small particle sizes and local lattice distortions can be characterized in a laboratory system. The present invention obtains data acquisition routines from scanning 3DXRD by translating and rotating the sample using a stage, and from Laue microdiffraction by focusing the beam to a smaller spot diameter using a polychromatic X-ray source. , obtained the concept of measuring the Laue diffraction pattern of a polychromatic beam. When scanning the sample by translation at different rotations of the sample, individual voxels within the sample can be illuminated and detected in multiple recordings, and the crystal orientation within each voxel is determined based on the above recordings. You can decide. By repeating the scan and rotation for each layer of the sample, a 3D image of the sample can be reconstructed.

Adapting the above technique to a laboratory setting using a laboratory X-ray source may require the use of focusing optics to focus the X-ray source to a spot diameter of less than 30 μm. be.

By focusing the X-ray source to a spot diameter of less than 30 μm, particles in the 1-30 μm range can be characterized, and the use of polychromatic X-rays allows the use of Laue diffraction techniques to detect local orientations. and lattice strains can be measured and the 3D volume reconstructed. The lower and upper limits of the particle size may depend on the specifications of the condensing optical component and the sample to be measured.

When using a polychromatic X-ray beam, such lattice strains can be reconstructed using Laue diffraction patterns, making it possible to measure local lattice strains within the particles in the sample. It could be possible. However, laboratory-based X-ray sources may not produce the necessary flux to use different apertures (used for synchrotron Laue microdiffraction) and therefore This technique needs to be combined with scanning 3DXRD techniques to locally resolve orientation and strain information.

Combining these techniques is not yet envisaged, as switching from Bragg diffraction to Laue diffraction is complex and it is clear that the present invention does not envisage synchrotron microdiffraction.

Conventional and non-traditional indexing methods may be used in the above method to index the Laue diffraction pattern. The latter may use machine learning methods or deep learning.

Accordingly, the present invention combines two synchrotron techniques in a novel and inventive manner to create a laboratory-based 3D scanning Laue microdiffraction system and method (Lab3DμXRD).

In US Pat. No. 9,383,324 (B2), the translation of the sample is only for alignment before data acquisition, not for data acquisition. The concentrating system of WO 2009/126868 (A1), which has only monochromatic X-rays or a limited range of discretization energies, is described in US Pat. No. 9,383,324 (B2). , it produces only X-rays that are not a continuous polychromatic spectrum, which is considered too low for DCT. DCT was originally designed based on a monochromatic synchrotron x-ray beam.

While the focusing system described in WO 2009/126868 (A1) is primarily for focusing monochromatic beams and usually soft X-rays (energy less than 10 keV), the present invention The system according to the invention uses focusing optics to produce focused hard polychromatic X-rays (energy less than 10 keV) with a continuous energy spectrum, which is particularly difficult to have with small spot diameters of less than 20-30 μm. Achieve parts.

In a preferred embodiment, the system may include a shield that can be placed between the radiation source and the sample and a beam stop that can be placed after the sample. This configuration is advantageous in having a beam stop after the sample to block the transmitted beam and thereby protect the detector if it is placed in the path of the transmitted beam. obtain. Having a shield can be advantageous because it blocks the direct beam from the radiation source that has not passed through the collection optics, thereby improving the contrast of the diffraction pattern.

In a preferred embodiment, the laboratory x-ray source is capable of producing a polychromatic beam with x-ray energy in the range of 5-150 keV.

In preferred embodiments, the focusing optics are capable of focusing the x-ray beam to a spot diameter of less than 20 μm, preferably less than 10 μm, more preferably less than 5 μm, or most preferably less than 1 μm.

It can be advantageous to have a spot size as small as the smallest particle to be measured in crystalline materials.

In preferred embodiments, the detector may be of the type photon counting, flat panel, scintillator based CCD or CMOS detector.

In preferred embodiments, the collection optic may be a double parabolic x-ray mirror optic, an ellipsoidal optic, a polycapillary optic, a Kirkpatrick-Baez mirror, or the like.

By using different focusing optics, the size of the spot diameter of the focused beam can be selected depending on the specifications and requirements of the sample and 3D characterization.

In a preferred embodiment, two or more detectors may be placed at different positions in the path of the diffracted X-rays, and the plurality of detectors have non-overlapping regions in the radial plane defined by the diffracted X-rays. You may do so.

In a preferred embodiment, the detector may be located 5-10 mm to 1 meter from the sample, and the collection optics may be located 20-50 mm from the sample (measured from the end of the optic to the sample). may be located in

In a preferred embodiment, the translation step along the first translation axis can be selected based on the beam diameter and the sample particle size. The translational interval may be within the beam spot diameter range of 1 to 30 μm or more.

In a preferred embodiment, the translation range may cover part or all of the longest side of the sample at different rotations. In other embodiments, the rotation and translation intervals and steps can be selected based on the gauge volume being characterized within the sample. In a preferred embodiment, the translation interval and range along the first translation axis may be the same for different rotations of the sample. However, in other embodiments, the translation spacing and range along the first translation axis may be different translation ranges and spacings for different rotations.

In such situations, the defined voxels may not be evenly distributed. This may be advantageous in situations, for example, where a hole is present in the sample, so that the hole is skipped in translation. In other embodiments, the translation steps may be the same for one rotation angle, but different for different rotation angles. For example, a 0 degree translation step may be in units of 1, and a 45 degree translation step may be in units of sqrt(2)/2. Alternatively, the translation steps may be pre-characterized at each revolution so as to skip translation steps where the beam is not directed into the sample.

In preferred embodiments, spatial resolution can be improved by translating the sample with a step size smaller than the focused beam spot diameter.

In preferred embodiments, the rotation may extend to a quarter turn, a half turn, or a full turn, although other rotation ranges are also contemplated. In preferred embodiments, the rotation interval may be about 1 to 90 degrees and may be the same for different rotations. In such embodiments, the sample is rotated several times, e.g., 7 times, at intervals of 0 degrees, 30 degrees, 60 degrees, 90 degrees, 120 degrees, 150 degrees, and 180 degrees to rotate each layer 7 times. Can be scanned twice. In some embodiments, the rotation interval may vary from rotation to rotation, such as a first rotation of 30 degrees and then a rotation of 60 degrees.

However, the translations and rotations may be in any range and spacing combination depending on the sample being characterized. This ensures that individual voxels within the sample are recorded more than once. Using this method, measurements can be selected for recording selected voxels with separate measurements.

In a preferred embodiment, Laue diffraction patterns are detected at different time intervals to generate a 4D image where time is the fourth dimension where the crystalline material can be exposed to any external stimulus.

In preferred embodiments, the indexing is of the type pattern matching, dictionary indexing, deep learning.

Gauge volume preferably refers to the volume within the sample being characterized.

Internal sample volume preferably means the volume within the sample that is illuminated by the beam during measurements.

Voxel preferably means a defined volume within a sample. The shape of the voxel may differ from the cubic element. Voxels may overlap.

Scanning preferably means translating the sample relative to the beam and taking new measurements along the scanning direction.

Range preferably means the distance/rotation angle between the first translation/rotation and the last translation/rotation. A step preferably means a change in distance/rotation.

By layer is preferably meant a virtually sliced segment of the sample.

Spot diameter preferably means the smallest size cross-sectional diameter in the beam.

Laboratory X-ray sources preferably mean machines and radiation sources used in laboratory settings and are negatively defined as not being synchrotron beams.

Indexing preferably involves identifying diffraction spots in a diffraction image, determining from which lattice planes of the particle (or voxel) those spots are diffracted, and thereby determining the crystallographic orientation of the particle (or voxel). means to decide.

Recording means detecting and storing the diffraction pattern from the detector, preferably for a single measurement.

Measurement preferably means exposure of the beam to the sample at a certain time, during which a diffraction pattern is recorded.

Hereinafter, the diffraction system and method according to the present invention will be described in detail with reference to the accompanying drawings. The drawings illustrate one way of carrying out the invention and are not to be construed as limiting other possible embodiments that fall within the scope of the appended set of claims.

FIG. 1A is a diagram illustrating one embodiment of the setup of the present invention. FIG. 1B is a diagram illustrating one embodiment of an internal sample volume illuminated by a focused beam. FIG. 1C shows an embodiment of the method according to the invention. FIG. 2 shows an embodiment of the invention in which the detector is placed at 90 degrees to the incident beam. FIG. 3 is a diagram illustrating an embodiment in which a diffraction pattern is detected using three detectors. FIG. 4 is a flowchart of an embodiment of the method according to the invention. FIG. 5 is a diagram illustrating one embodiment of a voxel.

FIG. 1A illustrates one embodiment of a laboratory-based 3D scanning X-ray Laue microdiffraction system 1 for characterization of crystalline materials. The system comprises a sample to be characterized 7 placed at a distance from the collection optics 4 and a laboratory X-ray source for producing a polychromatic X-ray beam 3 directed towards the collection optics 4. 2, a focusing optic 4 is arranged in the path of the beam 3 between the X-ray source 2 and the sample 7 and comprises a focused beam having a spot diameter of less than 30 μm at the imaging point located within the sample. generate. Sample 7 is preferably a crystalline material.

The focused beam 5 illuminates an internal sample volume 12 within the sample 7 and produces diffracted X-rays 8 from the entire illuminated internal sample volume 12 . Internal sample volume 12 is shown in FIG. 1B. In FIG. 1B, the shape of the focused beam 5 is cylindrical within the sample 7 due to the focal length being equal to or greater than the thickness of the sample 7 in some embodiments, while the interior sample volume illuminated The shape of 12 depends on the focused beam 5 illuminating the sample 7 and the relative position of the focal point within the sample and the magnitude of the focal length. In some embodiments, the sample thickness may be greater than the focal length and the beam diverges or converges within the sample so that the internal sample volume 12 is not cylindrical.

The diffracted X-rays 8 are detected and recorded by a detector 9 placed in the path of the diffracted X-rays 8 to detect the Laue diffraction pattern 13 of the internal sample volume 12 . This detector may be arranged in a transmissive or reflective geometry in one embodiment.

The detector 9 may in one embodiment be of a type such as a photon counting, flat panel, scintillator based CDD or CMOS detector.

The system further includes a stage 6 configured to support, rotate and translate the sample 7 relative to the focused beam 5 . The translation of the sample 7 by the stage 6 takes place in one embodiment in two directions perpendicular to each other. Stage 6 may consist of multiple components in some embodiments, such as a holder that holds the sample and a goniometer device that translates and rotates the holder.

The stage 6 is configured to rotate and translate the sample 7 at specific intervals and angles, and to scan the sample 7 in a grid pattern at different rotations of the sample 7, as shown in FIG. 1C.

The sample 7 can in one embodiment be translated along a first translation axis perpendicular to the beam and a second translation axis perpendicular to the beam. The desired gauge volume of the sample 7 is divided into layers along the second translational axis.

Thereby, the method consists of scanning the sample 7 layer by layer in a first translation axis perpendicular to the beam. In Figure 1C i) a top view of the sample 7 along the second translational axis is shown, where the sample 7 is scanned by translating the sample in 5 steps along the y-axis and Figure 1C The y-axis of corresponds to a first translational axis, the z-axis corresponds to a second translational axis, and the beam propagates along the x-axis.

Each of these translation steps corresponds to a separate measurement and recording of the Laue diffraction pattern 13 produced by the different internal sample volumes 12 being illuminated. In Figure 1C i), the majority of the X-ray beam is shown as a line, whereas the beam is shown for one beam in Figure 1C i) such that the internal sample volume within the sample is illuminated. like. Has a finite diameter.

As shown in ii) of FIG. 1C, after scanning the sample 7 along the y-axis, the sample 7 is rotated at a certain rotation interval and the sample 7 is scanned again along the y-axis, but in this procedure, The sample 7 is rotated 90 degrees and the sample 7 is scanned again along the y-axis, with a scan along the y-axis being performed after each rotation.

The rotation and translation steps are sample dependent. Each translation in the scanning step is a separate measurement, for example in the example shown in iii) of FIG. 1C, 5*2=10 measurements are performed for one layer of the sample 7.

In some embodiments, the data collection procedure includes directing the beam to the beginning of the translation range in a layer of the sample 7, recording the Laue diffraction pattern 13, and translating the sample 7 along the translation range in constant translation steps. , to record a new Laue diffraction pattern 13. If the translation spans the entire translation range, the sample 7 is rotated and the translation step is repeated. Although in this embodiment the axis of rotation is the z-axis, in some embodiments the axis of rotation may be independent of the first translation axis and the second translation axis.

Once the full rotation or desired range of rotation has been achieved, the sample 7 is translated along the second translation axis (in FIG. 1C the second translation axis is the z-axis) and the next layer is scanned. In some embodiments, the axes need not be perpendicular to each other.

By scanning the sample 7 with different rotations, each voxel 15 of the sample 7 can be illuminated during at least two measurements. A voxel 15 is a defined volume within the sample 7, as shown in iii) and iv) of FIG. 1C and in FIG.

By obtaining two or more recordings of the diffraction pattern 13 from the same voxel 15, the voxel 15 can be reconstructed by indexing the Laue diffraction pattern 13. Each voxel 15 within the sample can be indexed separately and a 3D image of the sample 7 can be reconstructed sequentially. By having smaller translation and rotation steps, each voxel 15 is illuminated with more measurements, improving resolution.

The rotation, translation range and step size are selected to ensure that each voxel 15 is recorded in at least two recordings, but the size of the voxel 15 is similarly selected using fixed translation and rotation steps and/or beams. Obviously, the choice can be made on the basis of diameter. Voxels 15 may vary in size within the sample and may even overlap, which occurs when the translational or rotational steps are non-linear. In some embodiments, the translation and rotation steps are selected to characterize only particular voxels within the gauge volume.

This means that signals from a shared internal volume from different measurements are indexed to extract information about the crystal orientation of each defined voxel. These shared volumes (i.e., voxels) are a priori based on translation and rotation, such as voxel 15 in iii) of Figure 1C, defined by translation measurement 3 with 0 degree rotation and translation measurement 3 with 90 degree rotation. can be determined.

Voxel 14 is reconstructed using a second measurement (from above) with a 0 degree rotation and a third measurement with a 90 degree rotation. Therefore, the measurement records used for the reconstruction of a particular voxel can be selected in the same way a priori before the measurement. If only voxels 14 and 15 have to be characterized, only three measurements are required. Therefore, the measurement procedure can be selected a priori based on the desired gauge volume and voxels within the gauge volume.

The translation steps and ranges and rotations are therefore selected based on the voxels within the gauge volume, ensuring that each voxel is illuminated in whole or in part during at least two measurements. The measurements may include metadata regarding translation and rotation steps to select the correct measurements to reconstruct the voxel. In FIG. 1C, the measurements can include metadata regarding scan position, rotational position, and layer position. These data may also include (first translational axis coordinates, second translational axis coordinates, rotational) data of the specimen 7, where the data is provided by the stage, such as by a positioning component within the stage 6. can do.

This method can be seen as a grid projected onto the plane of the sample 7, and then the grid points are moved spatially such that the same grid points are projected onto a newly rotated sample 7 with the same spatial coordinates. Rotate the sample while holding it in place. The particular rotational, translational step size and layer size are selected based on sample and beam geometry and thickness and other measurement factors.

For example, as shown in Figure 1C, if we perform 5 translations along the scanned y-axis and 3 layers with a rotation step of 90 degrees and a rotation range of 360 degrees, the number of measurements is 4*5*3= 60 and at least 5*5*3=75 individual voxels within the sample can be characterized within the sample 7. Some of these measurements may be null measurements.

The internal sample volumes 12 illuminated by the focused beams 5 may overlap in some embodiments and may not overlap in other embodiments. The number and overlap of these internal sample volumes may determine the resolution of the resulting 3D image.

Having such a system allows, in one embodiment, to characterize particles with a particle size of less than about 1 μm. The particular particle size that can be characterized may depend on the specifications of the collection optics 4 and the overlap between the selected internal sample volumes 12. The focusing optics 4 not only focuses the X-ray beam to the required diameter, but also increases the flux. The system thus combines the ideas of synchrotron scanning 3DXRD and synchrotron Laue microdiffraction in a laboratory setting.

In a preferred embodiment, the laboratory X-ray source 2 produces a polychromatic beam 3 with an X-ray energy in the range 5-150 keV. These energies can typically be generated by x-ray tubes that utilize metal objects, rotating anodes, liquid metal anodes, linearly accelerated radiation sources, and the like. In some embodiments, the radiation source 2 may be a synchrotron radiation source with a correspondingly higher flux. The disclosed systems and methods work equally well in a synchrotron setting as in a laboratory setting.

In one embodiment, the focusing optics 4 focuses the X-ray beam to a spot diameter of less than 20 μm, preferably less than 10 μm, more preferably less than 5 μm, and most preferably less than 1 μm. By condensing the beam, the intensity of the condensed beam 5 is simultaneously improved.

The selection of collection optics 4 depends on the particles to be characterized. As an example of this, when characterizing particles with a diameter of 1 to 5 μm, the focusing optics 4 best choose to focus the beam 3 to a spot diameter of less than 5 μm. In one embodiment, the focusing optics 4 may focus the beam 3 to a spot diameter of less than 1 μm so that particles of 1 μm diameter can be considered in an optimal manner.

In some embodiments, collection optics 4 are biparabolic x-ray mirror lenses, ellipsoidal optics, polycapillary optics, Kirkpatrick-Baez mirrors, and the like. By using a twin parabolic X-ray mirror, the beam 4 can be focused to a spot diameter of 5 μm or smaller.

The detector 9 can be placed at an angle to the incident beam as long as it is able to measure the diffracted light emitted from the internal sample volume 12. In one such embodiment, beam stop 10 is not required since no detector is placed in the path of transmitted beam 11. If the detector 9 is arranged in the path of the transmitted beam 11, a beam stop 10 can be arranged to block this transmitted beam.

As shown in FIG. 2, in one embodiment the detector 9 may be placed at an angle of 90 degrees to the focused beam 5. Thus, the detector can be placed in transmission geometry (0 degrees) or in reflection mode (90 degrees) or back projection mode (180 degrees) or any other angle. The system may include a shield 16 between the radiation source 2 and the sample 7 to block the direct beam from the radiation source 2.

As shown in FIG. 3, two or more detectors 9 may in one embodiment be placed at different positions in the path of the diffracted have non-overlapping areas in the radial plane. This creates a large detector area by arranging several small detectors 9 side by side.

In one embodiment, the detector 9 may be located at a position of 5-10 mm to 1 meter from the sample 7 and the focusing optics 4 may be located at a position of 20-50 mm from the sample 7 (optical (measured from the edge of the part to the sample). The exact placement of the detector 9 and optics 4 depends on the required spot diameter, optical working distance, detector pixel size, and other external factors.

A flow diagram illustrating a method of generating a 3D image of a sample is shown in FIG. The method consists, in a first step, of focusing a laboratory X-ray source 2 to a spot diameter of less than 30 μm and directing the focused beam 5 into the sample 7 to be characterized, thereby reducing the internal sample volume. 12 to generate diffracted X-rays 8. In this example, the beams 3, 5 are horizontal, so the first translation axis is horizontal and the second translation axis is vertical.

In a second step of the method, the sample 7 is scanned horizontally relative to the beams 3,5. Each translation corresponds to a new measurement where a Laue diffraction pattern is recorded. Once the sample 7 has been completely scanned horizontally, the sample 7 is rotated in a third step and is scanned horizontally again according to step 2.

Once the sample 7 has been completely rotated according to the rotation specifications, a fourth step is to vertically translate the sample 7, characterize a new layer of the sample 7, and repeat steps 2-4. This procedure is carried out until all the gauge volumes of the sample 7 selected for characterization have been scanned.

Once the sample 7 has been completely scanned, the recording of the diffraction pattern 13 can be used to index the individual voxels 15 of the gauge volume to reconstruct a 3D image of the sample. It is clear that steps 2, 3 and 4 are interchangeable and can be done in any order, that rotation can be done in any step, and that steps 2, 3 and 4 can be mixed. be.

The layer thickness and translation size can be preselected based on the voxels 15 to be characterized within the gauge volume of the sample 7.

In one embodiment, the internal sample volume 12 covers the volume of the sample 7 that can be illuminated by the focused beam 5 by rotating and translating the sample 7 at specific intervals. The scanned sample volume is also called the gauge volume, and all voxels within the gauge volume can be reconstructed.

If only a part of the sample needs to be characterized, only that part of the sample is covered by the scanning range while the sample is rotating. Thus, the gauge volume may be a portion of the sample or the entire sample.

In some embodiments, there are regions of overlap between the internal sample volumes 12 during scanning of the sample 7, and thus the sample 7 is translated during scanning with a step size smaller than the spot diameter of the focused beam 5. . The exact placement and number of internal sample volumes 12 depends on the specific requirements of the sample 7, such as desired resolution, coverage, sample size, etc.

In one embodiment, the rotation interval may be about 1-90 degrees, the translation interval may be a beam spot diameter size, such as 1-30 μm, and the layer thickness is such that the entire gauge volume is illuminated; The beam spot diameter may range from 1 to 30 μm to ensure that all of the internal sample volume 12 is the gauge volume.

The recorded diffraction pattern 13 is indexed when sufficient internal sample volume 12 is illuminated by the focused beam such that the diffraction pattern 13 from each voxel to be characterized is recorded by at least two measurements. A 3D image of the grain structure of sample 7 is reconstructed. This procedure is performed by indexing the pattern separately for each voxel and reconstructing the 3D volume by interpolating the differently indexed voxels.

Indexing, in one embodiment, may be pattern matching, dictionary indexing, or may be performed by using deep learning methods or other types of trained networks such as AI, neural networks, etc. .

When sample 7 is exposed to external stimuli, sample 7 may change its structure and properties over time. Therefore, by detecting Laue diffraction patterns at different time intervals for the same internal sample volume, a 4D of the sample can be constructed. This allows the crystalline material to be monitored and inspected under external stimulation.

In conclusion, the invention may include one or more of the following items.
i. - a condensing optical component (4);
- a sample to be characterized (7) placed at a distance from the focusing optics (4);
- a laboratory X-ray source (2) for producing a polychromatic X-ray beam (3);
- the focusing optics (4) are arranged in the path of the beam (3) between the X-ray source (2) and the sample (7), with a spot diameter of less than 30 μm at the imaging point in the sample (7); producing a focused beam (5) having diffracted X-rays ( 8) generate
- a stage (6) for holding a sample (7), the stage (6) being configured to rotate and translate the sample (7) relative to the focused beam (5);
- a laboratory-based 3D scanning X-ray Laue for characterizing crystalline materials, comprising: a detector (9) configured to detect a Laue diffraction pattern (13) of the diffracted X-rays (8); Microdiffraction system (1).
ii. - focusing a laboratory X-ray source (2) to a spot diameter of less than 30 μm in the sample (7) to produce a focused beam (5);
- defining a first translation axis perpendicular to the beam (5);
- defining a second translational axis perpendicular to the first translational axis and the beam (5);
- defining one or more layers within a predetermined gauge volume of the sample (7) along a second translational axis;
- scanning each layer of the sample (7) by translating the sample (7) at specific intervals along a first translational axis and recording the resulting diffraction pattern at each translation step;
- in more than one rotation, such that each layer of the sample (7) is scanned in a different rotation of the sample (7) and the Laue diffraction pattern from each voxel (15) is recorded in at least two recordings; irradiating each voxel (15) in the layer;
said layer is scanned by translating the sample (7) to the next layer along a second translational axis;
- A method for producing 3D orientation imaging of a crystalline material, comprising: indexing a recorded Laue diffraction pattern (13) to reconstruct a 3D image of the grain structure of a sample (7).

Although the invention has been described in connection with particular embodiments, it should in no way be construed as limited to the examples presented. The scope of the invention is set forth in the accompanying set of claims. In the context of the claims, the term "comprising" or "comprises" does not exclude other possible elements or steps. Further, references such as "a" and "an" should not be construed as excluding a plurality. The use of reference signs in the claims with respect to elements shown in the drawings shall not be construed as limiting the scope of the invention. Furthermore, individual features recited in different claims may be combined to advantage; the recitation of these features in different claims does not exclude that a combination of the features is not possible but advantageous.

1. Laboratory-based 3D scanning X-ray Laue microdiffraction system2. Laboratory X-ray source 3. Polychromatic X-ray beam4. Concentrating optics 5. Focused beam 6. Stage 7. Sample 8. Diffraction X-ray9. Detector 10. Beam stop 11. Transmitted beam 12. Internal sample volume 13. Laue diffraction pattern 14. Another voxel 15. Voxel 16. shield

Claims (15)

a condensing optical component (4);
a sample to be characterized (7) located at a distance from the focusing optics (4);
a laboratory X-ray source (2) for producing a polychromatic X-ray beam (3);
The focusing optics (4) are arranged in the path of the beam (3) between the X-ray source (2) and the sample (7), and the focusing optics (4) are arranged in the path of the beam (3) between the generating a focused beam (5) with a spot diameter of , generates diffracted X-rays (8),
a stage (6) for holding the sample (7), the stage configured to rotate and translate the sample (7) at predetermined intervals and angles with respect to the focused beam (5); (6) and
a detector (9) configured to detect a Laue diffraction pattern (13) of said diffracted X-rays (8); Microdiffraction system (1). between the sample (7) and the radiation source (2) to block the beam (3) directly from the radiation source that does not pass through the sample (7) and/or the focusing optics (4). 2. The system according to claim 1, wherein a beam stop (10) for blocking the transmitted beam (11) is arranged behind the shield (16) arranged between. 3. The system of claim 1 or 2, wherein the laboratory X-ray source produces a polychromatic beam with an X-ray energy in the range of 5 to 150 keV. Any of claims 1 to 3, wherein the focusing optics (4) focuses the X-ray beam to a spot diameter of less than 20 μm, preferably less than 10 μm, more preferably less than 5 μm, or most preferably less than 1 μm. or the system described in item 1. 5. A system according to any preceding claim, wherein the detector (9) is of the type photon counting, flat panel, scintillator based CCD or CMOS detector. Any of claims 1 to 5, wherein the focusing optic (4) is a double parabolic X-ray mirror optic, an ellipsoidal optic, a polycapillary optic, a Kirkpatrick-Baets mirror, or the like. or the system described in item 1. Two or more detectors (9) are arranged at different positions in the path of said diffracted X-rays (8), said plurality of detectors (9) being arranged in a radial plane defined by said diffracted X-rays (8). 7. A system according to any one of claims 1 to 6, having non-overlapping areas within the system. The detector (9) is placed at a position of 5-10 mm to 1 meter from the sample (7), and the condensing optical component (4) is placed at a position of 20-50 mm from the sample (7) (the optical 8. System according to any one of claims 1 to 7, arranged at the end of the part (4) to the sample (7). focusing a polychromatic X-ray beam (3) produced by a laboratory X-ray source (2) to a spot diameter of less than 30 μm in a sample (7) to produce a focused beam (5);
defining a first translational axis perpendicular to the beam (5);
defining a second translational axis perpendicular to the first translational axis and the beam (5);
defining one or more layers within a predetermined gauge volume of the sample (7) along the second translational axis;
scanning each layer of the sample (7) by translating the sample (7) along the first translational axis at specific intervals and recording the resulting diffraction pattern at each translation step; hand,
Each layer of the sample (7) is scanned in a different rotation of the sample (7), and the Laue diffraction pattern from each voxel (15) is recorded in at least two recordings. irradiating each voxel (15) in the layer;
the layer is scanned by translating the sample (7) to the next layer along the second translation axis;
indexing the recorded Laue diffraction pattern (13) to reconstruct a 3D image of the grain structure of the sample (7). The translation step along the first translation axis is selected based on the beam diameter and the particle size of the sample, and the translation range is a portion of the longest side of the sample (7) in the plurality of rotations. 10. The method of claim 9, wherein the method covers the entire longest piece. 11. A method according to claim 9 or 10, wherein the rotation interval is about 1 to 90 degrees and the translation interval is in the range 1 to 30 μm, corresponding to the beam spot diameter. 12. A method according to any of claims 9 to 11, wherein the rotation interval is the same for different rotations or varies from rotation to rotation, such as first a 30 degree rotation and then a 60 degree rotation. 13. A method according to any of claims 9 to 12, wherein the rotation is extended to a quarter, half or full rotation of the sample or some other range of rotations. 14. A method according to any of claims 9 to 13, wherein the Laue diffraction patterns are detected at different time intervals to generate a 4D image in which time is the fourth dimension of the crystalline material. 15. A method according to any of claims 9 to 14, wherein the indexing is of the type pattern matching, dictionary indexing, deep learning.

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